Hydroxyl-contained alicyclic epoxy resin and preparation method thereof

A technology of epoxy resin and hydroxyl ester, which is applied in the field of hydroxyl-containing alicyclic epoxy resin and its preparation, can solve the problems of low reactivity, decreased thermal performance of epoxy resin, and color introduction, and achieve chemical modification performance Good, increase curing activity, excellent heat resistance and mechanical properties

Inactive Publication Date: 2012-05-30
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the epoxy group of the alicyclic epoxy resin is on the rigid ring, the reactivity is relatively low. During the curing process, an accelerator needs to be added to accelerate its reaction with the curing agent, but at the same time it will produce compatibility and bring color and a series of questions
In addition, the traditional cycloaliphatic epoxy resin has only epoxy groups, and its chemical modification can only be achieved by consuming epoxy groups, but this method will reduce the crosslinking density of the cured epoxy resin, thereby Causes a decline in the thermal properties of epoxy resins

Method used

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  • Hydroxyl-contained alicyclic epoxy resin and preparation method thereof
  • Hydroxyl-contained alicyclic epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 100g (0.73mol) of pentaerythritol, 229g (1.46mol) of methyl 3,4-epoxycyclohexanecarboxylate and 0.16g of isopropyl titanate, and react at 150°C for 3 hours under the protection of an inert gas. The methanol produced by the reaction is discharged with the inert gas during the reaction, and finally the hydroxyl-containing alicyclic epoxy resin is obtained, IR: 3450cm-1(-OH), 1726cm-1(-COO-).

[0022] Take the above 10g of hydroxyl-containing alicyclic epoxy resin and 2.57g of p, p’-diaminodiphenylmethane and mix thoroughly, and cure according to the program of 90°C / 3h+150°C / 2h+180°C / 2h. The impact strength of the cured product is 20kJ m-2 (the impact strength is measured by a pendulum impact tester, the sample is a cuboid with a size of 60×6×4.5mm3), Tg 140°C (after the sample is cured, it is ground into powder , tested with a Perkin-Elmer DSC-2C differential scanning calorimeter produced by PE Company in the United States, N2 atmosphere, and the heating rate is 20 °C...

Embodiment 2

[0024] Mix 100g (0.75mol) of trimethylolpropane, 233g (1.50mol) of methyl 3,4-epoxycyclohexanecarboxylate and 3.3g of dibutyltin dilaurate at 80°C under the protection of an inert gas After 12 hours of reaction, the methanol produced by the reaction was discharged with the inert gas during the reaction, and finally a hydroxyl-containing alicyclic epoxy resin was obtained.

[0025] Take the above 10g of hydroxyl-containing alicyclic epoxy resin and 8.79g of methyl hexahydrophthalic anhydride, mix thoroughly, and cure according to the program of 90°C / 3h+150°C / 2h+180°C / 2h. The impact strength of the cured product is 20kJ·m-2 (the test method is the same as above), and the Tg is 145°C (the test method is the same as the above).

Embodiment 3

[0027] Mix 100g (0.75mol) trimethylolpropane, 233g (1.50mol) methyl 3,4-epoxycyclohexanecarboxylate and 1.6g sodium acetate, and react at 110°C for 5 hours under the protection of an inert gas , The methanol produced by the reaction is discharged with the inert gas during the reaction, and finally the hydroxyl-containing alicyclic epoxy resin is obtained.

[0028] Take the above 10g of hydroxyl-containing alicyclic epoxy resin and 7.0g of hexahydrophthalic anhydride and mix thoroughly, and cure according to the program of 120°C / 3h+150°C / 3h+200°C / 3h. The impact strength of the cured product is 21kJ·m-2 (the test method is the same as above), and the Tg is 150°C (the test method is the same as the above).

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Abstract

The invention discloses a hydroxyl-contained alicyclic epoxy resin and a preparation method thereof. The preparation method comprises the following steps of: mixing a hydroxyl compound with 3,4-epoxycyclohexane carboxylic acid methyl ester; then adding a catalyst and evenly mixing; and heating at 80-150 DEG C for reaction for 3-8 hours in the presence of inert gas shield to obtain the hydroxyl-contained alicyclic epoxy resin. According to the invention, an accelerator is not needed to be added in the solidifying process of the hydroxyl-contained alicyclic epoxy resin, and moreover, the chemical modification performance is good. Solidified products have good heat resistance and mechanical property.

Description

technical field [0001] The invention relates to the field of epoxy resins, in particular to a hydroxyl-containing alicyclic epoxy resin and a preparation method thereof. Background technique [0002] Cycloaliphatic epoxy resins have low viscosity, high heat resistance, and anti-ultraviolet radiation, and have broad application prospects. Since the epoxy group of the alicyclic epoxy resin is on the rigid ring, the reactivity is relatively low. During the curing process, an accelerator needs to be added to accelerate its reaction with the curing agent, but at the same time it will produce compatibility and bring color And so on a series of questions. In addition, the traditional cycloaliphatic epoxy resin has only epoxy groups, and its chemical modification can only be achieved by consuming epoxy groups, but this method will reduce the crosslinking density of the cured epoxy resin, thereby Lead to a decline in the thermal performance of the epoxy resin. Contents of the inv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02
Inventor 刘伟区马松琪
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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